The persistence of fluoroquinolone antibiotics such as ciprofloxacin in aquatic environments poses a serious challenge, as conventional treatment processes are often ineffective and their accumulation promotes antimicrobial resistance. To address this, BaTiO3/TiO2 heterojunction photocatalysts were synthesized via in-situ hydrothermal and ex-situ physical mixing routes and characterized to correlate their physicochemical properties with photocatalytic activity. XRD, FTIR, and XPS confirmed the coexistence of tetragonal BaTiO3 and anatase TiO2 phases, with synthesis-dependent variations in oxygen vacancies and surface chemistry. Morphological analysis by FE-SEM and FE-TEM revealed rod-like TiO2 growth on BaTiO3 in hydrothermal composites, while physically mixed samples exhibited more uniform surface decoration. BET analysis showed that hydrothermal products provided higher surface areas and mesoporosity, whereas physical mixtures contained irregular pores caused by particle aggregation. Optical characterization by UV–Vis-DRS suggested slight bandgap narrowing in hydrothermal composites, attributable to stronger interfacial coupling. Photocatalytic tests were performed under UV irradiation using a 400 W UV lamp at 365 nm, with ciprofloxacin at 40 ppm and pH 4 and a catalyst loading of 1 g/L. The physically mixed composites, particularly BaTiO3/TiO2–40P, achieved the highest degradation efficiency (96.4%) with kapp of 0.0185 min–1 within 180 min. These results indicated that although hydrothermal synthesis improves textural properties, the defect-rich interfaces and favorable charge trapping in physically mixed composites yield superior photocatalytic efficiency. This study emphasized the importance of interfacial engineering and synthesis control in developing efficient ferroelectric-semiconductor photocatalysts for wastewater treatment applications.
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